#------------------------------------------------------------------------------
#$Date: 2012-02-24 17:13:23 +0000 (Fri, 24 Feb 2012) $
#$Revision: 34330 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/03/4000373.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4000373
_journal_name_full 'Chemistry of Materials'
_journal_year    2004
_chemical_formula_moiety          'C44 H102 Mo2 N2 O16 P2 Si2'
_chemical_formula_sum             'C44 H102 Mo2 N2 O16 P2 Si2'
_chemical_formula_weight          1225.28
_symmetry_cell_setting            'monoclinic'
_space_group_IT_number           12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_[local]_cod_cif_authors_sg_H-M  C2/m
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x, y, -z'
 'x+1/2, y+1/2, z'
 '-x+1/2, y+1/2, -z'
 '-x, -y, -z'
 'x, -y, z'
 '-x+1/2, -y+1/2, -z'
 'x+1/2, -y+1/2, z'
_cell_length_a                    15.7641(13)
_cell_length_b                    20.947(2)
_cell_length_c                    10.0739(8)
_cell_angle_alpha                 90.00
_cell_angle_beta                  106.907(2)
_cell_angle_gamma                 90.00
_cell_volume                      3182.8(4)
_cell_formula_units_Z             2
_cell_measurement_temperature     129(2)
_cell_measurement_reflns_used     2610
_cell_measurement_theta_min       1.75
_cell_measurement_theta_max       24.7
_exptl_crystal_description        prism
_exptl_crystal_colour             red
_exptl_crystal_size_max           0.22
_exptl_crystal_size_mid           0.16
_exptl_crystal_size_min           0.14
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.279
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1300
_exptl_absorpt_coefficient_mu     0.538
_exptl_absorpt_correction_type    'empirical'
_exptl_absorpt_correction_T_min   0.59185
_exptl_absorpt_correction_T_max   0.96223
_exptl_absorpt_process_details    'Blessing, 1995'
_diffrn_ambient_temperature       129(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device        'Bruker SMART CCD'
_diffrn_measurement_method        \w-scans
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             7116
_diffrn_reflns_av_R_equivalents   0.0518
_diffrn_reflns_av_sigmaI/netI     0.0685
_diffrn_reflns_limit_h_min        -18
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -23
_diffrn_reflns_limit_k_max        23
_diffrn_reflns_limit_l_min        -11
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_theta_min          1.66
_diffrn_reflns_theta_max          24.69
_reflns_number_total              2697
_reflns_number_observed           2046
_reflns_observed_criterion        >2sigma(I)
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme
 'calc w=1/[\s^2^(Fo^2^)+(0.0669P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     'fixed'
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          2697
_refine_ls_number_parameters      175
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0661
_refine_ls_R_factor_obs           0.0437
_refine_ls_wR_factor_all          0.1103
_refine_ls_wR_factor_obs          0.1027
_refine_ls_goodness_of_fit_all    0.974
_refine_ls_goodness_of_fit_obs    1.051
_refine_ls_restrained_S_all       0.974
_refine_ls_restrained_S_obs       1.051
_refine_ls_shift/esd_max          0.000
_refine_ls_shift/esd_mean         0.000
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_thermal_displace_type
 _atom_site_occupancy
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_group
Mo1 Mo 0.07309(3) 0.0000 0.51483(5) 0.0156(2) Uani 1 d S .
P1 P 0.0000 0.13917(7) 0.5000 0.0194(4) Uani 1 d S .
Si1 Si 0.24666(11) 0.0000 0.7909(2) 0.0301(5) Uani 1 d S .
N1 N 0.0827(3) 0.0000 0.3272(4) 0.0177(11) Uani 1 d S .
O1 O 0.1434(2) 0.0000 0.7149(4) 0.0167(9) Uani 1 d S .
O2 O 0.2760(3) -0.0807(3) 0.8485(6) 0.0184(12) Uani 0.50 d P .
O2A O 0.2798(3) -0.0376(2) 0.9273(5) 0.0182(12) Uani 0.50 d P .
O3 O 0.2986(2) 0.0000 0.6750(4) 0.0244(10) Uani 1 d S .
O4 O 0.0843(2) 0.10002(12) 0.5310(3) 0.0192(6) Uani 1 d . .
O5 O -0.0113(2) 0.18349(13) 0.3705(3) 0.0294(8) Uani 1 d . .
C1 C 0.0249(4) 0.0000 0.1853(6) 0.0271(15) Uani 1 d S .
H1A H -0.0371(4) 0.0000 0.1860(6) 0.041 Uiso 1 calc SR .
H1B H 0.0365(4) -0.0382 0.1371(6) 0.041 Uiso 0.50 calc PR .
H1C H 0.0365(4) 0.0382 0.1371(6) 0.041 Uiso 0.50 calc PR .
C2 C 0.1757(4) 0.0000 0.3294(6) 0.030(2) Uani 1 d S .
H2A H 0.2135(4) 0.0000 0.4257(6) 0.045 Uiso 1 calc SR .
H2B H 0.1880(4) 0.0382 0.2820(6) 0.045 Uiso 0.50 calc PR .
H2C H 0.1880(4) -0.0382 0.2820(6) 0.045 Uiso 0.50 calc PR .
C3 C 0.2579(3) -0.1109(2) 0.9495(5) 0.0354(12) Uani 1 d . .
C4 C 0.2610(7) -0.1881(5) 0.9173(11) 0.043(3) Uiso 0.50 d P .
H4A H 0.2207(7) -0.1974(5) 0.8251(11) 0.064 Uiso 0.50 calc PR .
H4B H 0.2425(7) -0.2123(5) 0.9874(11) 0.064 Uiso 0.50 calc PR .
H4C H 0.3215(7) -0.2003(5) 0.9203(11) 0.064 Uiso 0.50 calc PR .
C4A C 0.2809(7) -0.1426(5) 0.8267(11) 0.046(3) Uiso 0.50 d P .
H4A1 H 0.2311(7) -0.1376(5) 0.7424(11) 0.069 Uiso 0.50 calc PR .
H4A2 H 0.2924(7) -0.1882(5) 0.8461(11) 0.069 Uiso 0.50 calc PR .
H4A3 H 0.3339(7) -0.1224(5) 0.8132(11) 0.069 Uiso 0.50 calc PR .
C5 C 0.1632(3) -0.1081(2) 0.9499(5) 0.0408(13) Uani 1 d . .
H5A H 0.1245(3) -0.1076(2) 0.8541(5) 0.061 Uiso 1 calc R .
H5B H 0.1534(3) -0.0693(2) 0.9977(5) 0.061 Uiso 1 calc R .
H5C H 0.1496(3) -0.1457(2) 0.9980(5) 0.061 Uiso 1 calc R .
C6 C 0.3226(4) -0.1119(3) 1.0895(6) 0.063(2) Uani 1 d . .
H6A H 0.3829(4) -0.1137(3) 1.0810(6) 0.095 Uiso 1 calc R .
H6B H 0.3119(4) -0.1495(3) 1.1403(6) 0.095 Uiso 1 calc R .
H6C H 0.3157(4) -0.0732(3) 1.1400(6) 0.095 Uiso 1 calc R .
C7 C 0.3898(4) 0.0000 0.6769(7) 0.032(2) Uani 1 d S .
C8 C 0.4531(4) 0.0000 0.8236(7) 0.041(2) Uani 1 d S .
H8A H 0.4334(4) 0.0317 0.8799(7) 0.062 Uiso 0.50 calc PR .
H8B H 0.5130(4) 0.0107 0.8204(7) 0.062 Uiso 0.50 calc PR .
H8C H 0.4535(4) -0.0424 0.8649(7) 0.062 Uiso 0.50 calc PR .
C9 C 0.3944(6) 0.0717(5) 0.6193(10) 0.033(2) Uiso 0.50 d P .
H9A H 0.3799(6) 0.1025(5) 0.6827(10) 0.050 Uiso 0.50 calc PR .
H9B H 0.3517(6) 0.0760(5) 0.5270(10) 0.050 Uiso 0.50 calc PR .
H9C H 0.4543(6) 0.0802(5) 0.6132(10) 0.050 Uiso 0.50 calc PR .
C9A C 0.4110(7) 0.0444(5) 0.5834(10) 0.035(2) Uiso 0.50 d P .
H9A1 H 0.4041(7) 0.0880(5) 0.6136(10) 0.053 Uiso 0.50 calc PR .
H9A2 H 0.3710(7) 0.0377(5) 0.4898(10) 0.053 Uiso 0.50 calc PR .
H9A3 H 0.4724(7) 0.0377(5) 0.5826(10) 0.053 Uiso 0.50 calc PR .
C10 C 0.0583(3) 0.2211(2) 0.3332(5) 0.0413(13) Uani 1 d . .
C11 C 0.1179(4) 0.2547(2) 0.4586(6) 0.053(2) Uani 1 d . .
H11A H 0.0824(4) 0.2835(2) 0.4976(6) 0.079 Uiso 1 calc R .
H11B H 0.1628(4) 0.2793(2) 0.4310(6) 0.079 Uiso 1 calc R .
H11C H 0.1471(4) 0.2230(2) 0.5286(6) 0.079 Uiso 1 calc R .
C12 C 0.1094(4) 0.1759(3) 0.2686(7) 0.071(2) Uani 1 d . .
H12A H 0.0686(4) 0.1551(3) 0.1879(7) 0.106 Uiso 1 calc R .
H12B H 0.1385(4) 0.1434(3) 0.3367(7) 0.106 Uiso 1 calc R .
H12C H 0.1542(4) 0.1998(3) 0.2391(7) 0.106 Uiso 1 calc R .
C13 C 0.0040(4) 0.2692(3) 0.2281(6) 0.069(2) Uani 1 d . .
H13A H -0.0281(4) 0.2976(3) 0.2742(6) 0.104 Uiso 1 calc R .
H13B H -0.0385(4) 0.2463(3) 0.1526(6) 0.104 Uiso 1 calc R .
H13C H 0.0439(4) 0.2945(3) 0.1903(6) 0.104 Uiso 1 calc R .
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
Mo1 0.0176(3) 0.0148(3) 0.0129(3) 0.000 0.0022(2) 0.000
P1 0.0223(9) 0.0117(8) 0.0211(8) 0.000 0.0014(7) 0.000
Si1 0.0154(9) 0.0574(13) 0.0158(9) 0.000 0.0017(7) 0.000
N1 0.021(3) 0.023(3) 0.010(2) 0.000 0.005(2) 0.000
O1 0.011(2) 0.021(2) 0.018(2) 0.000 0.004(2) 0.000
O2 0.018(3) 0.017(3) 0.018(3) 0.002(3) 0.002(2) 0.000(2)
O2A 0.016(3) 0.019(3) 0.015(3) 0.002(3) -0.002(2) 0.001(2)
O3 0.014(2) 0.041(3) 0.017(2) 0.000 0.003(2) 0.000
O4 0.014(2) 0.0170(15) 0.024(2) -0.0007(12) 0.0018(13) -0.0019(11)
O5 0.032(2) 0.021(2) 0.029(2) 0.0095(13) -0.0009(14) -0.0027(14)
C1 0.021(3) 0.047(4) 0.012(3) 0.000 0.003(3) 0.000
C2 0.021(4) 0.049(4) 0.016(3) 0.000 0.000(3) 0.000
C3 0.037(3) 0.038(3) 0.026(3) -0.003(2) 0.001(2) 0.012(2)
C5 0.037(3) 0.044(3) 0.040(3) 0.020(2) 0.008(2) -0.005(2)
C6 0.046(4) 0.088(5) 0.043(4) 0.033(3) -0.007(3) -0.010(3)
C7 0.025(4) 0.045(4) 0.025(4) 0.000 0.006(3) 0.000
C8 0.018(4) 0.057(5) 0.044(5) 0.000 0.001(3) 0.000
C10 0.043(3) 0.031(3) 0.046(3) 0.020(2) 0.005(3) -0.014(2)
C11 0.047(3) 0.041(3) 0.058(4) 0.022(3) -0.005(3) -0.017(3)
C12 0.089(5) 0.061(4) 0.082(5) 0.015(4) 0.056(4) -0.017(4)
C13 0.065(4) 0.057(4) 0.064(4) 0.046(3) -0.015(3) -0.021(3)
_cod_database_code 4000373